Dispersion



Aug. l1, 1931. F. zwlLGMEYER 1,817,958

DISPERSION med Aug. 21, 192e E Zw/ ai/wEv/Ee, y

Patented Aug. 11, 1931 UNITED STATES Y FRITHJ'OF ZWILGMEYER, OF BUFFALO, NEW YORK, ASSIGNOR TO NATIONAL AN ILINE @c CHEMICAL COMPANY INC., F NEW YORK, N. Y., A CORPORATION OF NEW YORK PATENT or-'FlcE DISPERSION Application led August 21, 1926. Serial No. 130.626.

This invention relates to the dispersion of aggregated systems and an apparatus therefor, and more particularly relates to the formation of liquidliquid disperse systems or emulsions.

In effecting a chemical reaction between two or more reagents or substances wherein one or more of them are insoluble or immiscible in a solution of the others, the

reaction is often facilitated and more easily brought about by adding the insoluble or immiscible reagent as an emulsion, or in a highly dispersed state in a liquid medium, to the remaining substances.

For example, in' the production of dyestuffs by coupling a diazo compound into diphenylamine, the latter is usually present as an insoluble body. For instance, in the reparation of prearation of the dyestuff nown as Metanil ellow by coupling diphenylamine with diazotised metanilic acid, a common procedure consists in dissolving the diphenylamine in strong sulfuric acid and reprecipitating it in a finely divided state therefrom in the presence of diazotised metanilic acid. This procedure, however, introduces an adulterant which requires neutralization and has further deleterious effects on the coupling reaction. These disadvantages are avoided and the time cycle considerably reduced by liquefying the diphenylamine and forming an emulsion thereof with water and then contacting the emulsion with the diazotised metanilic acid.

According to the present invention, dispersion is accomplished by placing the materials in a container, preferably in admixture with a dispersing agent, where they are suitably agitated and causing them in the fluid state to flow from the container as a narrow stream, which is forced, preferably under elevated pressure, in a zigzag or sinuous course until dispersion is accomplished.

In the accompanying drawing, Fig. 1 is a diagrammatic sectional view of a modified form of a conductor in which 'the zigzag ow takes place.

vided with a heating means such as a burner 2, beneath the bottom thereof, which may be supplemented or replaced by a heatmg coil 3 through which steam may be passed. One or more sides of the container may be heat msulated as shown. Stirring, for. obtaming a uniform mixture of the materlals, may be carried on by any suitable form of .mechanical agitator; but in the smaller s1zes of apparatus, particularly, air or steam directed into the mixture by a plpe 5 is found sufficient. Pressure may be exerted upon the charge by air, steam or any other suitable medium admitted through plpe 5 or through a valve controlled ipe 15, as may be desirable, and indicated y a gauge, for example, gau e 16.

The mixture is wlth rawn in a narrow stream from the container through a valve controlled line 6. Extending across the outlet of this line is a jet 7 communicating w1th a valved line 8 feeding air steam or any other suitable medium thereto. A chamber 9 encloses the 'et and a sinuous conductor or pipe 10 lea s from the chamber. The shape given the conductor presents a series of baiiies 11 to the oncoming fluld. An equivalent arrangement is a straight conductor rovided with baflies 12 on opposite sides o and inclined in the direction of iiow toward a median plane as shown in Fig. 2; these are staggered suiiciently to form a continuous, sinuous passage. The baiies may lie in the same axial plane or in planes in angular relation to one another. The emerging dispersed system is directed as desired.

In the manufacture of azo dyestufs derived from diphenylamine, for example, Metanil Yellow, the aggregated stem in the container comprises molten iphenyl- `amine to which water, together with a small percentage of soap and soda ash as emulsifiersor dispersing a ents, is added as a disperslon medium. he mixture is agitated to obtain uniformity and is drawn throu h the line 6. Steam under ressure from t e line 8 forces the mixture rom the chamber 9 and impels it throu h the conductor or emulsifier l0, where, ue to the repeated impingements or sharp collisions of the mixture against the baies, it results an emulsion. For example, a well agltated mixture at a temperature of about -90 C., and comprised of about 10 parts by weight of molten diphenylamlne, 14 parts sodlum carbonate, 14: parts of potash; soap and 170 parts Water, Will produce a satisfactory dispersion, i. e., an emulsion having a milky appearance, u on being forced at a rate of approximate y 700 to 800 cc. per minute through a pipe 10, as shown, of about 12 to 14 inches in length, and one fourth inch in diameter, and having six sections disposed in zigzag fashion, the angle of intersection being about 120 C. Other emulsifying or dispersing agents than soap may be used, e. g., dextrine, gs1ue, Turkey red oil, etc.' Thelr presence a1 1n the f ormation of an emulslon chiefly by stabilizing it.

This emulsion is directed to the surface of a solution of a diazo body, such as diazotized metanilic acid, contained in an agitated vat 13 wherein the coupling takes place. Instead of a direct passage from the emulsiler 10 to the vat 13, the emulsion can be directed to an intermediate vat for coolin and then distributed to the vat 13.

arious other means may be substitutedV be denitely determined and their mixture,l

with or Without the dispersing agent, made uniform before impelling the resulting mixture through the emulser, it is evident that the charge need not include the dispersion medium and the latter may be utilized as the mpelling agent. In place of a jet, an atomizer or other impelling means, it 1s possible to apply suiiicient pressure upon the mixture in the container as to impart a How of its contents throiihgh the sinuous conductor at a velocity su cient to give adequate impingement and the desired disperslon. Furthermore, the container may be omitted entirely, and the reagent and the dispersion medium, in admixture or separately, and with or Without the presence of a dlspersing agent, may be supplled to the sinuous conductor, with the interposition of a jet or atomizer if desired, either one or both being impelled by suiicient force to cause the required dis ersion. When a reagent is normally a soli as in the illustration given above, its emulsification is made possible by the application of heat, or other suitable means, to bring it into the liquid condition; and such a change in state can be caused to take lace in a container, as shown, with or wit out the addition of the dis ersion medium. Where heat is applied Wit out the admixture of the dispersion medium, there should be a suiicient supply of heat to avoid solidiication of the reagent during the process of dispersion; and heat may be supplied by the partial or complete vaporization of the dispersion medium, which may be usedin that condition to impel or to atomize the liquefied solid.

I claim:

l. A process for dispersing av substance which comprises mixing the substance in a fluid state with a dispersing agent and a dispersion medium, and causing impingement of a narrow stream of the resulting mixture.

2. A process for dispersin a substance which is normally solid at ordinary temperature which comprises combining the substance in the melted state with a dispersion medium and passing the combination under pressure through a zigzag conduit so that the melted material and dispersion medium collide sharply with the conduit and unite to form a dispersed system.

3. A process for dispersing a substance Which comprises causing an impingement of the substance in admixture with a dispersion medium, a dispersing agent and steam.

4f. A process for dispersing a substance which comprises mixing Athe substance in a Huid state With a dispersion medium and an emulsifying agent, and passing the resulting mixture with steam through a sinuous conductor to cause impingement and produce a dispersed system.

5. A process for the emulsification of a diphenylamine which comprises mixing the molten diphenylamine with water and an emulsifying agent and passing the mixture in the fluid state under pressure in contact with steam throughv a sinuous conductor and in sharp collisions therewith.

6. A process for the emulsiiication of diphenylamine which comprises passing an admixture of diphenylamine, Water, soap and sodium carbonate in contact With steam through a zigzag conduit.

7. A process for the emulsiiication of a diphenylamine Which comprises emulsifying the diphenylamine bod by -causing its impingementin the liqui state in admixture with a dispersion medium.

8. A `process for the emulsification of a diphenylamine which comprises emulsifying diphenylamine by causing its impingement in the liquid state in admixture with Water and soft soap, and in contact with steam.

9. A process for dispersing a substance which comprises mixing the substance in a fiuid state with a dispersion medium and a dispersing agent and passing the resulting mixture under pressure through a sinuous conguctor to cause sharp collisions therewit 10. A process for dispersi a substance which comprises passing an a mixture containing the substance, a dispersion medium and a dipersing agent under pressure through a sinuous conductor to cause sharp collisions therewith.

In testimony whereof I aiiix my si ature.

FRITHJOF ZWILGME ER. 

